CN109735827A - A kind of solid polymer carbon source electrochemical deposition technique and device - Google Patents
A kind of solid polymer carbon source electrochemical deposition technique and device Download PDFInfo
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- CN109735827A CN109735827A CN201910191998.0A CN201910191998A CN109735827A CN 109735827 A CN109735827 A CN 109735827A CN 201910191998 A CN201910191998 A CN 201910191998A CN 109735827 A CN109735827 A CN 109735827A
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Abstract
It mainly includes gas outlet pipe, Zuo Guansai, DC power supply, high temperature furnace, heating tube, right pipe close, gas inlet pipe, inert gas quantitative output device, conductive rod, clamping device, exhaust gas processing device, insulated enclosure circle, matrix, quartz boat and solid polymer etc. that the present invention, which discloses a kind of solid polymer carbon source electrochemical deposition technique and device, device,.The technology of the present invention replaces the gases such as methane using polyolefins such as solid polymer PE or PVC as carbon source, at low cost, safer；During preparing graphene, the influence of voltage electric field is added, improves graphene growth and prepares quality；Voltage electric field is provided to clamping device by the way of external power supply, while laser heating, which can be used, decomposes solid polymer polyolefin based materials.The technology can be applied to the preparation of conductive coating, grapheme material, directly can also carry out graphene conductive coating to device, increase raw material by the performances such as conduction in original performance applications, can expand the application field of material.
Description
Technical field
The present invention relates to high performance carbon cellulosic material preparation field more particularly to a kind of solid polymer carbon source electrochemical depositions
Technology and device.
Background technique
In recent years, the research of high performance carbon cellulosic material is quite active, and diversified nano-carbon material emerges one after another, mainly
Based on the materials such as carbon fiber, graphene, carbon nanotube, fullerene.Wherein, graphene and multi-layer graphene material are in material supply section
, micro-nano technology, the energy, biomedicine and drug delivery etc. are with important application prospects, it is considered to be a kind of future
Revolutionary material
Currently, being directed to graphene preparation mainly using chemical vapor deposition (CVD) method, this method application precursor gas
Body (carbon source) is mainly methane (CH4), ethylene (C2H4), acetylene (C2H2) etc. several hydrocarbon gas, stayed by carbon source molecule dehydrogenation
Lower carbon atom is grown in metallic substrates or nonmetal base material prepares graphene or other carbon structures, such as patent
CN104123999A etc..However methane gas belongs to inflammable gas, misoperation is easily caused danger during the preparation process, risk
Larger higher cost, and the graphene grown has apparent fold, limits the preparation and application of high-quality graphene.Therefore,
The carbon source material and high-quality preparation method for finding the new low cost of one kind are problems in urgent need to solve.
Summary of the invention
In view of the above problems, the present invention proposes a kind of solid polymer carbon source electrochemical deposition technique.The present invention is with poly- second
The solid polyolefins hydro carbons materials such as alkene (PE), polyvinyl chloride (PVC) are as carbon source, the sky being passed through in inert gas discharge heating device
Gas is prepared in inert gas shielding environment, so that c h bond and C-C key in the materials such as PE is broken using high-temperature heating cracking
It splits, finally obtains active atoms of carbon and short carbon chain, carbochain and carbon atom are in SiO2, gradually deposit on the matrixes such as Ni, Cu, grow system
Standby graphene or equadag coating out.Meanwhile voltage or electric field is added in innovation during the preparation process, can promote carbochain and carbon atom
Stablize on matrix, high quality growth.The inventive technique method are as follows: matrix and solid polymer carbon source are put into and add by the first step
In heat pipe, duct occlusion is heated, to guarantee subsequent isolation air；Second step, heating tube vacuumize and are passed through inert gas；Third
Step opens DC power supply power supply, using laser or high temperature stove heating, makes the high-temperature heating cracking of solid polymer carbon source, is swum
From carbon atom or short carbon chain, the accelerating velocity of laser or high temperature stove heating is 30~50 DEG C/min, final heating temperature model
Enclosing is 800~1000 DEG C, 30~50 DEG C/min of cooling rate；4th step closes high temperature furnace, closes inert gas and quantitatively exports dress
It sets, opens left pipe close, take out graphene or equadag coating matrix.
Related application equipment predominant gas discharge pipe of the present invention, Zuo Guansai, DC power supply, high temperature furnace, heating tube, right pipe
Plug, gas inlet pipe, inert gas quantitative output device, conductive rod, clamping device, exhaust gas processing device, insulated enclosure circle, base
Body, quartz boat and solid polymer etc..Wherein, it is connected between inert gas quantitative output device and heating tube using heat-resistant tube,
Heating tube is placed in high temperature furnace；Matrix and quartz boat or corundum boat are placed in heating tube, fill solid polymerization in quartz boat
Object carbon source PE, matrix and quartz boat are placed on the center of heating tube, the two maximum distance < 10cm；Heating tube both ends equipped with
Pipe close (sealing-plug) is sealed to form inert gas shielding space in heating process；Clamping device leads to inside heating tube
It crosses conductive thin stick or conductor wire is connected to external power supply, power supply is furnished with resistance, prevents short circuit.
During the preparation process, inert gas is vacuumized and be passed through first, is then added using high temperature furnace electric heating or laser
The mode of heat heats heating tube.Wherein, the accelerating velocity of heating is 30~50 DEG C/min, and final heating temperature range is 800
~1000 DEG C, 30~50 DEG C/min of cooling rate；The heating speed and the rate of heat addition of laser heating are depending on laser heating power.
Step mode in the invention is external mode, and left pipe close or right pipe close are provided with micropore, and power supply connects conductive rod
Or conductor wire passes through micropore and enters in heating tube, voltage or electric field is provided to matrix, between micropore and conductive rod or conductor wire
Can be high-temperature resistant rubber material also it be other materials equipped with insulated ring, plays insulation and gas-tight body drain goes out.It is powered external
Can also by heating tube, heating tube can aperture be perhaps equipped with the conductive thin stick of branch pipe or conductor wire through hole or branch pipe enter plus
In heat pipe, voltage or electric field are provided.Insulated enclosure circle also is provided between hole or branch pipe and conductive rod or conductor wire.
During the preparation process, using clamping device come fixing base, clamping device is conductive metal material.Conductive rod or gold
Belong to line and use copper or other conductive metals, the melting temperature of conductive metal material is greater than the attainable upper limit temperature of heating method institute
Degree.In heating tube heating and temperature-fall period, certain voltage is applied to basis material by conductive rod or conductor wire, in voltage
Under the action of electric current, the quickly and orderly of high-quality graphene and coating is promoted to grow preparation.Matrix makes after having very thin coating
It obtains matrix and is provided with electric conductivity or electric conductivity raising, under the action of electric field, deposition efficiency and quality are all improved.
Clamping device in the invention is removable to be changed to two electrode plates, generates electricity among two electrode plates by external power supply
, basis material is placed in two electrode plates, promotes growth preparation of the graphene on matrix under electric field action.Wherein, two electricity
The distance and electric field level of pole plate are adjustable.
The carbon source polymeric material applied in heating tube is solid-state, such as PE, PP and PVC material at normal temperature.
Polymer material additional amount requires to be adjusted according to practical preparation, and polymer is placed on the high temperature-resistant vessels such as quartz boat or corundum boat
In, it is put into heating tube before heating.
The adaptable depositing base of the technology has SiC matrix, Ni matrix, Cu matrix etc., applies in graphene prepared above
Layer, class equadag coating.The technology can apply to carbon fiber substrate and glass fiber matrix simultaneously, carry out carbon fiber and glass fibre
Surface it is modified, promote thermal conductivity.
The present invention proposes a kind of solid polymer carbon source electrochemical deposition technique, which includes: (1) benefit
The polyolefins such as solid polymer PE or PVC are used to replace the gases such as methane as carbon source, it is at low cost, it is safer；(2) it is mentioning
A kind of new electrochemical deposition mode is gone out, during preparing graphene, the influence of voltage electric field is added, it is raw to improve graphene
Long preparation quality；(3) present invention proposes a kind of new electrochemical deposition implementing device, electric to providing by the way of external power supply
Piezoelectric field, while laser heating, which can be used, decomposes solid polymer polyolefin based materials.The technology can be applied to conductive coating,
The preparation of grapheme material directly can also carry out graphene conductive coating to device, make raw material in original performance applications
Increase the performances such as conduction, expands the application field of material.
Detailed description of the invention
Fig. 1 is a kind of solid polymer carbon source electrochemical deposition technique application equipment of the present invention.
Fig. 2 is a kind of solid polymer carbon source gas phase deposition technology heating tube schematic internal view of the present invention.
In figure, 1- gas outlet pipe, the left pipe close of 2-, 3- DC power supply, 4- high temperature furnace, 5- heating tube, the right pipe close of 6-, 7- gas
Body access tube, 8- inert gas quantitative output device, 9- conductive rod, 10- clamping device, 11- exhaust gas processing device, 12- insulation
Sealing ring, 13- matrix, 14- quartz boat, 15- solid polymer.
Specific embodiment
Related application equipment of the present invention mainly includes gas outlet pipe 1, Zuo Guansai 2, DC power supply 3, high temperature furnace 4, heating
Pipe 5, right pipe close 6, gas inlet pipe 7, inert gas quantitative output device 8, conductive rod 9, clamping device 10, exhaust gas processing device
11, insulated enclosure circle 12, matrix 13, quartz boat 14 and solid polymer 15 etc., as shown in Figure 1.Inert gas quantitatively exports dress
It sets 8 and right pipe close 6 is connected by gas inlet pipe 7, and inert gas is passed into heating tube 5 according to certain flow velocity, heat
Pipe 5 is placed in high temperature furnace 4, and conductive rod 9 is deep into heating tube 5 by left pipe close 2, as shown in Figure 2, metal clamping device 10
It is connected externally to power supply 3 by conductive rod 9, for solid polymer 15 including PE, PVC etc., solid polymer 15 is put into quartz boat
14,10 fixing base 13 of clamping device connects gas outlet pipe 1 on the left of heating tube 5, and the gas that gas outlet pipe 1 is discharged imports
Into exhaust gas processing device 11, vent gas treatment is carried out.
The present invention is intended to provide the manufacturing method of a kind of more orientation stacking carbon fibre composites and carbon fiber woven cloth.Tool
Body embodiment are as follows: (1) select a certain amount of polymer P E, PVC etc. to be put into quartz boat or corundum boat 14, be then placed in
The center of heating tube 5.(2) 10 fixing base 13 of clamping device is used, Zuo Guansai 2 and right pipe close 6 are installed in heating tube 5,
Matrix 13 is put in heating tube 5, and Zuo Guansai 2 and right pipe close 6 play sealing function to heating tube.(3) pass through gas outlet pipe 1
To being vacuumized in heating tube 5, air is taken away, inert gas quantitative output device 8 will by inert gas access tube 7, pipe 7
Inert gas is passed into heating tube 5 by certain flow.Gas outlet pipe 1 connects exhaust gas processing device 11, is discharged at collection
Manage tail gas.(4) it opens power supply 3 to power, high temperature furnace 4 presses 5~30 DEG C/min heating rate after starting and heats heating tube 5, reaches most
Cool down after high-temperature by the rate of temperature fall of 10~50 DEG C/min.(5) high temperature furnace 4 is closed, inert gas quantitative output device is closed
8, left pipe close 2 is opened, graphene or equadag coating matrix are taken out.
Claims (8)
1. a kind of solid polymer carbon source electrochemical deposition technique, it is characterised in that: the first step, by matrix and solid polymer carbon
Source is put into heating tube, heats duct occlusion, to guarantee subsequent isolation air；Second step, heating tube vacuumize and are passed through indifferent gas
Body；Third step opens DC power supply power supply, using laser or high temperature stove heating, according to certain heating speed after high temperature furnace starting
Degree heating cools down after reaching maximum temperature according to certain cooling rate, makes the high-temperature heating cracking of solid polymer carbon source, obtains
Free carbon atom or short carbon chain；4th step closes high temperature furnace, closes inert gas quantitative output device, opens left pipe close,
Take out graphene or equadag coating matrix.
2. a kind of solid polymer carbon source electrochemical deposition technique according to claim 1, it is characterised in that: laser or height
The accelerating velocity of warm stove heating is 30~50 DEG C/min, and final heating temperature range is 800~1000 DEG C, cooling rate 30~50
℃/min。
3. a kind of solid polymer carbon source electrochemical deposition technique according to claim 1, it is characterised in that: solid polymerization
Object carbon source is polyolefin.
4. a kind of solid polymer carbon source electrochemical depositer, it is characterised in that: mainly include gas outlet pipe, Zuo Guansai,
DC power supply, high temperature furnace, heating tube, right pipe close, gas inlet pipe, inert gas quantitative output device, conductive rod, clamping dress
It sets, exhaust gas processing device, insulated enclosure circle, matrix, quartz boat and solid polymer carbon source, wherein inert gas quantitatively exports
It is connected between device and heating tube using heat-resistant tube, heating tube is placed in high temperature furnace；Matrix and quartz boat are placed in heating tube,
Solid polymer carbon source is filled in quartz boat, matrix and quartz boat are placed on the center of heating tube；Heating tube both ends equipped with
Pipe close, pipe close are divided into left pipe close and right pipe close, are sealed to form inert gas shielding space in heating process；Clamping device exists
Inside heating tube, and external power supply is connected to by conductive thin stick or conductor wire, power supply is furnished with resistance；Left pipe close or right pipe
Plug is provided with micropore, and DC power supply connection conductive rod or conductor wire pass through micropore and enter in heating tube, to matrix provide voltage or
Electric field is equipped with insulated ring between micropore and conductive rod or conductor wire；Clamping device fixing base, clamping device are metallic conduction material
Material.
5. a kind of solid polymer carbon source electrochemical depositer according to claim 4, it is characterised in that: matrix and stone
Both English boats maximum distance is less than 10cm.
6. a kind of solid polymer carbon source electrochemical depositer according to claim 4, it is characterised in that: logical heating tube
Aperture is perhaps equipped with the conductive thin stick of branch pipe or conductor wire through hole, and perhaps branch pipe enters in heating tube and provides voltage or electric field.
7. a kind of solid polymer carbon source electrochemical depositer according to claim 4, it is characterised in that: clamping device
It changes as two electrode plates, electric field is generated among two electrode plates by external power supply, basis material is placed in two electrode plates, in electricity
Promote growth preparation of the graphene on matrix under field action.
8. a kind of solid polymer carbon source electrochemical depositer according to claim 4, it is characterised in that: matrix includes
SiC matrix, Ni matrix, Cu matrix or carbon fiber, glass fibre.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910191998.0A CN109735827A (en) | 2019-03-14 | 2019-03-14 | A kind of solid polymer carbon source electrochemical deposition technique and device |
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| CN201910191998.0A CN109735827A (en) | 2019-03-14 | 2019-03-14 | A kind of solid polymer carbon source electrochemical deposition technique and device |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102400109A (en) * | 2011-11-11 | 2012-04-04 | 南京航空航天大学 | Method for growing large area of layer-number-controllable graphene at low temperature through chemical vapor deposition (CVD) method by using polystyrene solid state carbon source |
| CN103708444A (en) * | 2013-12-20 | 2014-04-09 | 上海中电振华晶体技术有限公司 | Preparation method and equipment of graphene film |
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- 2019-03-14 CN CN201910191998.0A patent/CN109735827A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102400109A (en) * | 2011-11-11 | 2012-04-04 | 南京航空航天大学 | Method for growing large area of layer-number-controllable graphene at low temperature through chemical vapor deposition (CVD) method by using polystyrene solid state carbon source |
| CN103708444A (en) * | 2013-12-20 | 2014-04-09 | 上海中电振华晶体技术有限公司 | Preparation method and equipment of graphene film |
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